EP4292994A1 - Zementiermaterial mit niedrigem ph-wert und herstellungsverfahren dafür - Google Patents

Zementiermaterial mit niedrigem ph-wert und herstellungsverfahren dafür Download PDF

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Publication number
EP4292994A1
EP4292994A1 EP22893945.0A EP22893945A EP4292994A1 EP 4292994 A1 EP4292994 A1 EP 4292994A1 EP 22893945 A EP22893945 A EP 22893945A EP 4292994 A1 EP4292994 A1 EP 4292994A1
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EP
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Prior art keywords
value
parts
cementing material
low
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22893945.0A
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English (en)
French (fr)
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EP4292994A4 (de
Inventor
Ju Wang
Liang Chen
Wei Lu
Weiquan ZHAO
Jianhua Zhou
Hongsu Ma
Xingguang ZHAO
Jian Liu
Xiang Zhang
Xin Lu
Yufang Wang
Zengzeng REN
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Institute of Water Resources and Hydropower Research
Beijing Research Institute of Uranium Geology
Original Assignee
China Institute of Water Resources and Hydropower Research
Beijing Research Institute of Uranium Geology
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Application filed by China Institute of Water Resources and Hydropower Research, Beijing Research Institute of Uranium Geology filed Critical China Institute of Water Resources and Hydropower Research
Publication of EP4292994A1 publication Critical patent/EP4292994A1/de
Publication of EP4292994A4 publication Critical patent/EP4292994A4/de
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
    • C04B2103/0094—Agents for altering or buffering the pH; Ingredients characterised by their pH
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00017—Aspects relating to the protection of the environment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00112—Mixtures characterised by specific pH values
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/00258—Electromagnetic wave absorbing or shielding materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00767—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00862—Uses not provided for elsewhere in C04B2111/00 for nuclear applications, e.g. ray-absorbing concrete
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Definitions

  • the present invention relates to the technical field of building materials, and in particular to a low-pH value cementing material and a preparation method therefor.
  • the safe disposal of a large amount of high-level radioactive waste generated during the development and utilization of nuclear energy is the last link in the nuclear industry chain and is crucial to the sustainable development of the nuclear industry. Because the high-level radioactive waste can remain radioactive for thousands to hundreds of thousands of years, the internationally recognized safe, reliable and long-term disposal plan is to build a high-level radioactive waste disposal repository in a rock mass 500 m to 1000 m underground. High-level radioactive waste is permanently isolated from the human living environment through artificial barrier systems such as storage tanks and bentonite.
  • the pH value of the cement-based cementing materials used to plug cracks and backfill chambers in the construction of the disposal repository must be reduced to less than or equal to 11 within a certain period of time after the material is hardened.
  • cement clinker It is well known that the main components of cement clinker are tricalcium silicate, dicalcium silicate, tricalcium aluminate, and tetracalcium aluminoferrite, which, when hydrated, generate a large amount of calcium hydroxide, the solution is alkaline.
  • a water dissolution method may be used to measure a pH value of the cementing material prepared by taking common Portland cement as a base material, namely, the material cured under standard conditions is dried in the shade, crushed and ground, a sample is weighed, the sample and water (distilled water) are mixed according to a water-solid ratio of 10:1 at a temperature of 20 ⁇ 2 °C, then the mixture is stirred at a high speed for 30 min, and a pH value of filtrate is measured by a pH meter after the mixture is filtered by a dry filter paper.
  • the measured data and public literature reports show that the pH value of the common Portland cement is still about 12.5 within a few years, which cannot meet the requirements for the construction of a high-level radioactive waste disposal repository.
  • the main method to reduce the pH value of the cement-based cementing materials is to add active materials to consume calcium hydroxide generated during cement hydration or change cement clinker, so that no or less calcium hydroxide is generated during cement hydration .
  • Chinese Patent No. CN107311576A discloses a low-alkalinity ecological concrete and a preparation method therefor, wherein the low-alkalinity ecological concrete comprises the following components in parts by weight: 40-60 parts of sludge ceramsite, 15-30 parts of sulphoaluminate cement, 2-7.5 parts of a water-reducing admixture, 10-20 parts of fly ash, 7-15 parts of slag fine powder, 3-8 parts of plant ash, 1-5 parts of aluminum sulfate, and 10-25 parts of water.
  • the material has a pH value of less than 11, and has the same mechanical property as common concrete, and has biological applicability which is not available in common materials.
  • Chinese Patent No. CN107548949A discloses a low-alkalinity cementing material for plant-growing concrete and a preparation method therefor, wherein the low-alkalinity cementing material comprises the following components in parts by weight: 60-100 parts of superfine slag powder, 20-30 parts of Portland cement, 0-20 parts of a modified component, 5-20 parts of waste mortar, 0.05-0.5 parts of waste rubber particles, 0-1 parts of expanded perlite, and 0.1-2 parts of a water-reducing admixture.
  • the material takes silicate as an auxiliary cementing material, and the pH value of a cured soaking solution is 9.0-9.5, which can provide growth conditions for plants.
  • Chinese Patent No. CN101439939A discloses a low alkalinity cementing material for manufacturing concrete artificial fish reef and a preparation method therefor, wherein the material comprises the following components in parts by weight: 40-60 parts of blast furnace water quenching slag, 5-25 parts of fly ash or furnace slag and the like, 10-30 parts of natural dihydrate gypsum or anhydrite and the like, and 1-5 parts of ferric sulfate or ferrous sulfate and the like.
  • the material does not generate calcium hydroxide after hydration, and the prepared concrete can quickly have the same pH value as seawater on the surface in a natural sea area, which is beneficial to the reproduction of aquatic organisms.
  • Chinese Patent No. CN106242490A discloses a low-pH value superfine phosphoaluminate cement-based grouting material, wherein the material comprises the following components in parts by weight: 45-55 parts of phosphoaluminate cement, 25-35 parts of fly ash, 5-15 parts of slag, 5 parts of a dispersant, 0.5-1 parts of polycarboxylic acid water-reducing admixture, and 1 part of an expanding agent, wherein the prepared grouting material has a pH value of less than or equal to 11, has the characteristics of high fluidity and high grouting property, and has micro-expansibility.
  • the low alkalinity sulphoaluminate cement specified in the National Standard of Sulphoaluminate Cement (GB20472) is mainly made of sulfate cement, limestone, and gypsum, has an alkalinity pH value of less than or equal to 10.5 and the characteristics of low alkalinity.
  • the low-pH value cementing materials mainly use sulphoaluminate cement or a small amount of Portland cement as base materials.
  • the cementing materials which are generally accepted and used internationally still take common Portland cement with a long-term application history as a main base material.
  • the results of foreign research and practice have shown that the pH value of the cementing material prepared by adding a large amount of silica fumes (more than 40% by weight) into common Portland cement can be reduced to less than or equal to 11 at about day 150, and the pH value of the material is basically not changed when the fly ash or ground granulated blast furnace slag with the same proportion is singly added.
  • the specific surface area of the silica fumes is 80-100 times that of cement, and after the silica fumes are added in a large amount, a large amount of water-reducing admixture is required to be added for ensuring the fluidity, and the series problems of large viscosity, low early strength, high plastic shrinkage cracking risk, and the like of a cementing material are brought, consequently, the rock mass crack plugging and chamber backfilling effects of a disposal reservoir are influenced.
  • the present invention provides a low-pH value cementing material and a preparation method therefor.
  • the cementing material invented takes the common Portland cement which is generally accepted internationally as a main base material, which not only solves the problems of high viscosity, low early strength, high plastic shrinkage cracking risk, and the like caused by the fact that more than 40% of silica fumes are added in the cement in the prior art abroad, but also can adjust a speed of pH value reduction and the required age that the pH value is less than 11 and improve the mechanical property by changing the addition amount of the modified material in the cementing material, so that different requirements in the construction of high-level radioactive waste disposal repository are met.
  • the cementing material provides support for constructing an internationally advanced high-level radioactive waste disposal repository in China.
  • the present invention uses the following technical solutions.
  • the present invention provides a low-pH value cementing material, which comprises the following components in parts by weight: 60-65 parts of cement, 0-12 parts of aggregate, 25-35 parts of silica fumes, 3-6 parts of a pH value regulator, and 0.7-1.5 parts of a water-reducing admixture.
  • the pH value regulator comprises the following components: nano-silicon dioxide, anhydrous powdery calcium chloride, aluminum potassium sulfate dodecahydrate, and calcium stearate, wherein the nano-silicon dioxide, the anhydrous powdery calcium chloride, the aluminum potassium sulfate dodecahydrate, and the calcium stearate are in a mass ratio of 50-60:20-25:10-15:2-4.
  • the nano-silicon dioxide has a purity of greater than or equal to 99%, and the nano-silicon dioxide has a particle size of 15-30 nm; the anhydrous powdery calcium chloride has a purity of greater than or equal to 90%; the aluminum potassium sulfate dodecahydrate has a purity of greater than or equal to 99%; and the calcium stearate has a calcium content of 6% to 7%.
  • the cement is common Portland cement
  • the aggregate is fly ash or ground granulated blast furnace slag
  • the silica in the silica fumes has a content of not less than 95%
  • the water-reducing admixture is a naphthalene-based high-efficiency water-reducing admixture with a water reducing effect of not less than 20%.
  • the fly ash is of Grade I Class C and the ground granulated blast furnace slag is of Class S105.
  • the present invention further provides a preparation method for the low-pH value cementing material, which comprises the following steps:
  • the present invention provides a low-pH value cementing material, which comprises the following components in parts by weight: 60-65 parts of cement, 0-12 parts of aggregate, 25-35 parts of silica fumes, 3-6 parts of a pH value regulator, and 0.7-1.5 parts of a water-reducing admixture.
  • the low-pH value cementing material comprises 60-65 parts of the cement, preferably 61-64 parts, and more preferably 62-63 parts;
  • the pH value regulator comprises the following components: nano-silicon dioxide, anhydrous powdery calcium chloride, aluminum potassium sulfate dodecahydrate, and calcium stearate;
  • the mass ratio of the nano-silicon dioxide, the anhydrous powdery calcium chloride, the aluminum potassium sulfate dodecahydrate, and the calcium stearate is preferably 50-60:20-25:10-15:2-4, and more preferably 55-58:22-23:11-14:3.
  • the purity of the nano-silicon dioxide is preferably greater than or equal to 99%, and more preferably greater than or equal to 99.9%;
  • the particle size of the nano-silicon dioxide is preferably 15-30 nm, and more preferably 20-25 nm;
  • the purity of the anhydrous powdery calcium chloride is preferably greater than or equal to 90%, and more preferably greater than or equal to 95%;
  • the purity of the aluminum potassium sulfate dodecahydrate is preferably greater than or equal to 99%, and more preferably greater than or equal to 99.9%;
  • the calcium stearate preferably contains 6-7% of calcium, and more preferably contains 6.5% of calcium.
  • the cement is common Portland cement
  • the aggregate is fly ash or ground granulated blast furnace slag
  • the silica in the silica fumes has a content of not less than 95%
  • the water-reducing admixture is a naphthalene-based high-efficiency water-reducing admixture with a water reducing effect of not less than 20%.
  • the fly ash is Grade I Class C fly ash
  • the ground granulated blast furnace slag is Class S105 ground granulated blast furnace slag
  • the fluidity and the strength of the cementing material can be adjusted by adjusting the mixing proportion of the fly ash and the ground granulated blast furnace slag.
  • the present invention further provides a preparation method for the low-pH value cementing material, which comprises the following steps:
  • the addition amount of water is greater than or equal to 40% of the mass of the cement, the aggregate, the silica fumes, the pH value regulator, and the water-reducing admixture.
  • the humidity of the curing is greater than or equal to 95%; the curing temperature is 18-22 °C; the curing time is greater than or equal to 28 days.
  • the required age that the pH value of the cementing material is reduced to less than or equal to 11 is adjusted by adjusting the addition amount of the silica fumes and pH value regulator.
  • Example 1 60 parts of common Portland cement, 35 parts of silica fumes, 5 parts of a pH value regulator, and 1.5 parts of a water-reducing admixture; wherein the pH value regulator comprises nano-silicon dioxide, anhydrous powdery calcium chloride, aluminum potassium sulfate dodecahydrate, and calcium stearate in a mass ratio of 55:20:12:3
  • Example 2 60 parts of common Portland cement, 30 parts of silica fumes, 6 parts of fly ash, 4 parts of a pH value regulator, and 1.2 parts of a water-reducing admixture; wherein the pH value regulator comprises nano-silicon dioxide, anhydrous powdery calcium chloride, aluminum potassium sulfate dodecahydrate, and calcium stearate in a mass ratio of 50:21:12:
  • the preparation method of the cementing material described in Examples 1 to 3 and Comparative Examples 1 to 2 comprises the following steps:
  • the preparation method of the cementing material described in Example 4 to 5 comprises the following steps:
  • the method for measuring the pH value of the cementing materials described in Examples 1 to 5 and Comparative Examples 1 to 2 comprises the following steps:
  • the strength of the cementing materials described in Examples 1 to 5 and Comparative Examples 1 to 2 was measured according to the Method of testing cements-Determination of strength (GB/T17671), namely, 1 part of a cementing material, 3 parts of ISO standard sand, and 0.5 parts of water were used to prepare a cementing material, and the compressive strength of the specimen was measured after curing under standard conditions.
  • the hydrated products of the cementing material obtained by the present invention are all dense hydrated calcium silicate (C-S-H) gels, and Ca(OH) 2 crystals (hexagonal plates) are not found.
  • the low-pH value cementing material for the high-level radioactive waste disposal repository provided by the present invention can adapt to different parts and functional requirements by changing the ratio.
  • the cementing material in Example 1 can be used in a high-level radioactive waste disposal roadway plugging body which has high requirements on the reduction speed of the pH value of the material and low requirements on the strength; and the cementing material in Example 3 can be used in cracked rock grouting impervious materials which have low requirements on pH value reduction time but have high requirements on fluidity.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
EP22893945.0A 2022-04-24 2022-12-12 Zementiermaterial mit niedrigem ph-wert und herstellungsverfahren dafür Pending EP4292994A4 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202210451297.8A CN114656222B (zh) 2022-04-24 2022-04-24 一种低pH值胶凝材料及其制备方法
PCT/CN2022/138357 WO2023207125A1 (zh) 2022-04-24 2022-12-12 一种低pH值胶凝材料及其制备方法

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EP4292994A1 true EP4292994A1 (de) 2023-12-20
EP4292994A4 EP4292994A4 (de) 2024-07-10

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EP (1) EP4292994A4 (de)
CN (1) CN114656222B (de)
WO (1) WO2023207125A1 (de)

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Publication number Priority date Publication date Assignee Title
CN114656222B (zh) * 2022-04-24 2022-11-15 核工业北京地质研究院 一种低pH值胶凝材料及其制备方法
CN115537204A (zh) * 2022-09-20 2022-12-30 徐州工程学院 一种用于酸性土壤的生物碳改良剂的制备工艺及其应用
CN117069446B (zh) * 2023-08-07 2024-03-26 中国水利水电科学研究院 一种低pH混凝土及其制备方法和应用

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CN114656222B (zh) * 2022-04-24 2022-11-15 核工业北京地质研究院 一种低pH值胶凝材料及其制备方法

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CN114656222B (zh) 2022-11-15
CN114656222A (zh) 2022-06-24
EP4292994A4 (de) 2024-07-10

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